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Preparation and application of trifluorovinyl-ether-containing cyclosiloxane capable of direct heat curing

A technology of trifluorovinyl ether and cyclosiloxane, applied in the direction of silicon organic compounds, etc., can solve the problems of limited application, low mechanical properties, complex multi-component reaction process, etc., and achieve great application prospects and cross-linking degree. high effect

Active Publication Date: 2016-08-10
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Most of the above-mentioned monomers are difunctional monomers, which can form linear polymers with a certain molecular weight when heated and cross-linked. They are thermoplastic polymer materials, but the glass transition temperature of the material is low, the mechanical properties are low, and the application is limited. Other multifunctional materials need to be added. The monomer is modified, the multi-component reaction process is complicated and uncontrollable

Method used

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  • Preparation and application of trifluorovinyl-ether-containing cyclosiloxane capable of direct heat curing
  • Preparation and application of trifluorovinyl-ether-containing cyclosiloxane capable of direct heat curing
  • Preparation and application of trifluorovinyl-ether-containing cyclosiloxane capable of direct heat curing

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preparation example Construction

[0081] Preparation of Cyclosiloxane

[0082] The present invention also provides a method for preparing the cyclosiloxane, the method comprising the steps of: reacting the following monomer 1 and monomer 2 to obtain the cyclosiloxane as described in the first aspect of the present invention ;

[0083]

[0084] Or react with monomer 3 and monomer 4 as shown below to obtain cyclosiloxane as described in the first aspect of the present invention

[0085]

[0086] Wherein, the definition of each group is as described in the first aspect of the present invention.

[0087] The cyclic siloxane structure part is connected with the silane segment part containing trifluorovinyl ether phenyl group through hydrogen addition reaction. Preferably, the reaction is carried out in the presence of a catalyst selected from the group consisting of chloroplatinic acid, chloroplatinic acid-isopropanol solution, methylvinylsiloxane platinum complex, Karstedt catalyst, palladium complex, Rho...

Embodiment 1

[0127] Example 1 Preparation of 4-trifluorovinyl ether phenyldimethylsilane

[0128]

[0129] Under the protection of nitrogen, add 4.10 grams of magnesium strips, 26.08 grams of dimethylchlorosilane, a small amount of iodine and 100 milliliters of dry treated tetrahydrofuran into a dry 250 milliliter three-necked flask, stir and slowly add 35.10 grams of 4- Dissolve trifluorovinyl ether bromobenzene in 20 ml of tetrahydrofuran solution, heat slightly until the color of the system fades, react at room temperature for 15 hours after the dropwise addition, remove the solvent after filtering with diatomaceous earth, and collect the fraction 23.8 at 80°C / 20mba by distillation under reduced pressure g, yield 74%. 1 H NMR (400MHz, CDCl 3 ,δin ppm): 7.58~7.60(d,2H), 6.89~6.91(d,2H), 4.41-4.45(m,H), 1.20~1.24(t,6H). 19 F-NMR (376MHz, CDCl3, δin ppm): -119.35, -119.50, -119.60, -119.76, -126.15, -126.41, -126.44, -126.70, -133.56, -133.72, -133.72, -133.86, -134.01 .

Embodiment 2

[0130] Example 2 Preparation of 4-trifluorovinyl ether phenyldimethylchlorosilane

[0131] Under the protection of nitrogen, add 4.05 grams of magnesium strips, 34.85 grams of dimethyldichlorosilane, a small amount of iodine and 150 milliliters of dry treated tetrahydrofuran into a dry 250 milliliter three-necked flask, stir and slowly add 34.20 grams of 4 - Dissolve trifluorovinyl ether bromobenzene in 20 ml of tetrahydrofuran solution, heat slightly until the color of the system fades, react at room temperature for 20 hours after the dropwise addition, filter with diatomaceous earth, remove the solvent, and collect the fraction at 85°C / 20mba by vacuum distillation 22.47 g, 65% yield.

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Abstract

The invention provides preparation and application of trifluorovinyl-ether-containing cyclosiloxane capable of direct heat curing, particularly cyclosiloxane disclosed as Formula I (the groups are defined in the specification) and a curing product prepared from the cyclosiloxane. The cyclosiloxane preparation method is simple and controllable in processing; the monomer can be subjected to direct heat curing, is used for preparing high-performance thermosetting resins with high heat resistance, high weather resistance and low water absorptivity, has excellent and stable dielectric properties from low frequency to high frequency, and is suitable to be used as an electronic component packaging material in electronic and electric industries and used as a high-temperature-resistant adhesive in the fields of aerospace, national defense and the like.

Description

technical field [0001] The invention belongs to the field of organosilicon materials, and in particular relates to the preparation and application of a directly heat-curable cyclosiloxane containing trifluorovinyl ether. Background technique [0002] Organosilicon is a new type of chemical product with many varieties, excellent performance and wide application. Various silanes, siloxane intermediates and products such as silicone oil, silicone rubber and silicone resin made from them have been developed. Good thermal stability, weather resistance, electrical insulation and biological properties and other excellent properties, such as silicone resin can maintain stable and excellent dielectric properties in a wide range of temperature, humidity and frequency. Silicone products have been widely used in electronics, construction, automobiles, textiles, light industry, cosmetics, medical treatment, food and other industries, and are one of the fastest-growing varieties of new ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21C08G77/24C08K5/549
CPCC07F7/21C08G77/24C08K5/549
Inventor 房强王佳佳金凯凯孙晶朱芝田王元强
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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